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Method for efficiently preparing borohydride anion [RnH(4-n)B]<->

An anion and boron hydrogen technology, applied in chemical instruments and methods, boron halides, tetrafluoroboric acid, etc., can solve the problems of single product and poor applicability, and achieve the effect of wide applicability, low cost, and simple and efficient synthesis method

Inactive Publication Date: 2018-10-19
LESHAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ion exchange method can only synthesize BH 4 - anion salt, and the hydrogenation reduction method can only obtain monohydrogen triphenyl borohydride ammonium salt [Ph 3 HB] - , the above synthesis method product is single, applicability is poor, all can not be used for synthesizing other types [R n h 4-n B] - borohydride anion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Synthesis of 1,3-dimethylimidazolium boron tetrahydride

[0025] The reaction was carried out under argon protection. First, 0.5 g (2.7 mmol) of 1,3-dimethylimidazolium tetrafluoroborate was added to a 50 ml reaction tube with a vacuum stopcock, and then 10 g of dry anhydrous Dichloromethane solvent, 1,3-dimethylimidazolium tetrafluoroborate was completely dissolved under magnetic stirring. After complete dissolution, add 0.27mmol of boron tribromide as a catalyst and 5.4mmol of phenylsilane reducing agent to the reaction tube, stir and react at 35°C for 10 hours, and 1,3-dimethylimidazolium tetrafluoroborate is Completely reduced to 1,3-dimethylimidazolium boron hydride salt.

Embodiment 2

[0027] Synthesis of 1-Methyl-3-n-Butylimidazolium Hydrogenated Triphenylboron Salt

[0028] The reaction is carried out under the protection of high-purity nitrogen. First, in the reaction tube of 50ml with a vacuum cock, add the chlorinated 1-methyl-3-n-butyl imidazolium salt of 0.8g (4.6mmol), then add 4.6mmol of tris Phenylborane and 24g of dry chloroform were reacted for 1 hour under magnetic stirring to generate 1-methyl-3-n-butylimidazolium triphenylboron chloride. Then add 0.05mmol of triphenylborane as a catalyst to the above solution, 10mmol of diethylsilane reducing agent, stir and react at 40°C for 24 hours, 1-methyl-3-n-butylimidazole trichloride The phenyl boron salt is completely reduced to 1-methyl-3-n-butylimidazolium hydrogenated triphenyl boron salt.

Embodiment 3

[0030] Synthesis of 1-methyl-3-n-butylimidazolium trihydrophenyl boron salt

[0031] In Example 2, 4.6mmol of triphenylborane was replaced by 4.6mmol of dichlorophenylborane, and the rest of the steps were the same as in Example 2 to finally obtain the product 1-methyl-3-n-butylimidazole trihydrogen Phenyl boron salt.

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PUM

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Abstract

The invention discloses a method for efficiently preparing borohydride anion [RnH(4-n)B]<->, lewis acid RnX3-nB is taken as a catalyst, hydrogen containing silane is taken as a reducing agent, and various halogenated boron anionic ammonium salts [R'4N]<+>[RnX(4-n)B]<-> are reduced to corresponding borohydride anion ammonium salts [R'4N]<+>[RnH(4-n)B]<->. The method not only can prepare BH4<-> anionic salt and triphenyl borohydride ammonium salt [Ph3HB]<->, but also can synthesize various other types of borohydride anions [RnH(4-n)B]<->, the applicability is wide, and the synthesis method is simple and efficient. The method provides a novel way for the synthesis of the borohydride anion [RnH(4-n)B]<->.

Description

technical field [0001] The invention relates to the technical field of borohydride anion synthesis, in particular to a method for efficiently preparing borohydride anions [R n h 4-n B] - Methods. Background technique [0002] Sodium borohydride, potassium borohydride, lithium borohydride and other borohydride salts are the most common inorganic alkali metal borohydride salts, which are widely used in the reduction of aldehydes, ketones and carboxylic acid derivatives, plastic foaming agents, sewage treatment agents, Paper bleaching agent, hydrogen storage materials and other fields. There are many studies on alkali metal borohydride salts reported in the literature, but there are few related research reports on alkyl-containing borohydride salts. The introduction of an alkyl group into the anion or cation of borohydride can change the polarity of the compound, enhance its solubility and thus improve its reducing ability and reactivity. The introduction of an alkyl group ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02C07D233/58C07D213/127C07D213/18C01B6/13C01B35/06
CPCC01B6/13C01B35/061C01B35/063C07D213/127C07D213/18C07D233/58C07F5/027
Inventor 陈俏田冲任超聂万丽马克西姆徐鑫陈刚
Owner LESHAN NORMAL UNIV
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